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以双氧水(H_2O_2)为配合剂,采用混合萃取剂三烷基氧膦(TRPO)和磷酸三丁酯(TBP)从含WO3110~150 g·L~(-1)、Mo/WO_3(质量比)10%~15%的高钼钨酸铵溶液中萃取分离钨钼,负载有机相用NH_4HCO_3溶液选择性反萃Mo。在萃取-反萃取试验研究的基础上进行工业试验,利用kremser方程确定了平衡p H值、萃取级数和W,Mo萃取率之间的关系,提出了中间级加酸调p H值的2段式逆流萃取、2段式反萃取等新的工艺改进措施,在优化条件下长时间运转以考察新工艺的稳定性,并进行技术经济成本分析。结果表明:有机相组成(体积分数)为3%TRPO+70%TBP+27%磺化煤油,有机相流量为100 L·h-1,料液中含WO_3110~150 g·L~(-1),Mo/WO_3(质量比)10%~15%,优化试验条件下得到的萃余液中WO_3质量浓度为126~151 g·L~(-1),Mo质量浓度为0.0019~0.0120 g·L~(-1),Mo/WO_3质量比小于0.9×10~(-4);新工艺连续运转21个月,萃余液和反萃液质量稳定、有机相循环性能好、系统运行状况平稳;萃余液中Mo含量满足制备0级仲钨酸铵(APT)产品的需求。新工艺在处理高钼含钨溶液时,具有除Mo彻底、W收率高、Mo产品附加值高、成本低和清洁环保等优点。工业试验结果证明新工艺已具备产业化应用条件。
(H 2 O 2) was used as the complexing agent and the mixture was extracted with trialkylphosphine oxide (TRPO) and tributyl phosphate (TBP) from WO3110-150 g · L -1, Mo / WO_3 (mass ratio) 10% ~ 15% ammonium molybdate solution extraction and separation of tungsten and molybdenum, the organic phase loaded with NH_4HCO_3 selective stripping Mo. The industrial experiments were carried out on the basis of the extraction-back-extraction experiments. The relationship between the equilibrium p H value, the extraction order and the extraction rates of W and Mo was determined by the kremser equation. The mid-level acid-added p H value of 2 Stage counter-current extraction, two-stage stripping and other new process improvement measures, under the optimized conditions for a long time to examine the stability of the new process, and technical and economic cost analysis. The results showed that the composition of the organic phase (volume fraction) was 3% TRPO + 70% TBP + 27% sulfonated kerosene and the organic phase flow rate was 100 L · h -1. The feed solution contained WO3110-150 g · L -1 ) And Mo / WO_3 (mass ratio) of 10% ~ 15%. The optimum concentration of WO_3 in the raffinate was 126 ~ 151 g · L -1 and the mass concentration of Mo was 0.0019 ~ 0.0120 g · L ~ (-1), Mo / WO_3 mass ratio of less than 0.9 × 10 ~ (-4); the new process runs continuously for 21 months, the quality of raffinate and stripping liquid is stable, the organic phase has good cycle performance, ; The raffinate Mo content to meet the needs of the preparation of 0 level ammonium paratungstate (APT) products. The new process has the advantages of thoroughly removing Mo, high W yield, high added value of Mo products, low cost and environmental friendliness when processing the high-molybdenum tungsten solution. Industrial test results show that the new technology already has industrial application conditions.